Geo
Well-known member
i wouldnt let that sludge dry out without acidifying. ammonia can make some nasty stuff when dried with dissolved metals.
Went against my gut! Grrr...
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steyr223
Well-known member
Awesome stuff guys
I'm on the edge of my chair.... waiting! !
O wait I'll get the popcorn. :lol:
Steyr223 rob
I'm on the edge of my chair.... waiting! !
O wait I'll get the popcorn. :lol:
Steyr223 rob
Sorry for the slow update, I had a very busy weekend with my kids, but hey that's what it's about right! 
So the resulting button form the first drop with AR was just under -1.5g, a lot less then I estimated. After running the tests with ammonium, on the previous page in this thread, I washed everything real good, then dried and re-incinerated again, washed in hot Hcl (solution would turn a clear rusty orange with a negative stannous test) and water washes, then ran through AR, again with no success. During the AR process I would get positive stannous test, not a strong positive but still positive, in clean yellow solution, but by the time it had cooled down I would only get a faint purple stain with stannous and no purple stain at all by the time it was filtered and ready to drop.
So this makes me think a few things, 1. something is cause the gold to cement out 2. the unknown chlorides are locking up the gold and not allowing them to dissolve, 3. I possibly vaporized the gold during incineration. or 4. an obscure combination of all of the above.
So after all that I dried, re-incinerated, and hit the books reading everything I could find on tin compounds. I found out a lot about tin, a couple of things I found in common with the chemistry books I read, it didn't matter how old or new, is none of them really discussed how to convert tin(II) and tin(4) compounds back to elemental tin (if it's even possible) and they all stated how difficult it is to work with tin compounds in a solution.
So after I incinerated for the third time the remaining powder is now a light tan to off white in color, I washed it with water and ran a few test, all the proceeding tests were done with a small sample in a test tube.
1. added a 3ml of ammonium hydroxide, mixed, then heated thoroughly. poured off solution in to clean test tube, then added hcl one drop at a time: no reaction
2. re-acidified the powders in test tube 1 with Hcl, heated, then tested with stannous: negative stannous test
3. still test tube 1, added 8 drops of Hcl and 2 drops of HNo3, heated, cooled, then tested with stannous: positive stannous test
4. took a fresh sample and added 8 drops of Hcl and 2 drops HNo3, heated, tested with stannous: positive stannous test
So at this point I figured the last incineration was all it needed, so I put it all back into AR, and got the same results as the second time I ran it through AR, it would test negative for gold by the time it was ready to filter. I thought maybe my stannous was getting a little weak, I tested it against my standard solution many times just to make sure.
Back to the test tubes I took a fresh clean sample,
1. added a 3ml of water and a pinch of NaOH, heated gently: no reaction and no color change
The way I understood when I was ready about tin compounds, is that most stannic compounds are readily soluble in a concentrated alkali solution, which in theroy is what we deal with when we introduce tin into nitric acid. This creates a stannic/metastannic acid, then through incineration of the residue then creates stannic oxide, which should be soluble in concentrated sodium hydroxide. I am really trying to make an effort to better understand these chemical compounds/processes, so please correct me if my understanding is wrong.
At this point I am completely stumped, and have run out of ideas, so any thoughts any one else has are more then welcomed???
I had one of the same boards left that the pins came from, so I pulled just over a 1/2lb of them and ran through nitric. I used glondor's SS coffee filter basket technique he described in this thread to recover the foils from the chlorides. It worked perfectly, thanks glondor, I recovered and processed 2.18g from 0.65lbs of pins. I did this just make sure I wasn't going crazy.
I'll stop rambling now, thanks in advance for any input,
Chris
So the resulting button form the first drop with AR was just under -1.5g, a lot less then I estimated. After running the tests with ammonium, on the previous page in this thread, I washed everything real good, then dried and re-incinerated again, washed in hot Hcl (solution would turn a clear rusty orange with a negative stannous test) and water washes, then ran through AR, again with no success. During the AR process I would get positive stannous test, not a strong positive but still positive, in clean yellow solution, but by the time it had cooled down I would only get a faint purple stain with stannous and no purple stain at all by the time it was filtered and ready to drop.
So this makes me think a few things, 1. something is cause the gold to cement out 2. the unknown chlorides are locking up the gold and not allowing them to dissolve, 3. I possibly vaporized the gold during incineration. or 4. an obscure combination of all of the above.
So after all that I dried, re-incinerated, and hit the books reading everything I could find on tin compounds. I found out a lot about tin, a couple of things I found in common with the chemistry books I read, it didn't matter how old or new, is none of them really discussed how to convert tin(II) and tin(4) compounds back to elemental tin (if it's even possible) and they all stated how difficult it is to work with tin compounds in a solution.
So after I incinerated for the third time the remaining powder is now a light tan to off white in color, I washed it with water and ran a few test, all the proceeding tests were done with a small sample in a test tube.
1. added a 3ml of ammonium hydroxide, mixed, then heated thoroughly. poured off solution in to clean test tube, then added hcl one drop at a time: no reaction
2. re-acidified the powders in test tube 1 with Hcl, heated, then tested with stannous: negative stannous test
3. still test tube 1, added 8 drops of Hcl and 2 drops of HNo3, heated, cooled, then tested with stannous: positive stannous test
4. took a fresh sample and added 8 drops of Hcl and 2 drops HNo3, heated, tested with stannous: positive stannous test
So at this point I figured the last incineration was all it needed, so I put it all back into AR, and got the same results as the second time I ran it through AR, it would test negative for gold by the time it was ready to filter. I thought maybe my stannous was getting a little weak, I tested it against my standard solution many times just to make sure.
Back to the test tubes I took a fresh clean sample,
1. added a 3ml of water and a pinch of NaOH, heated gently: no reaction and no color change
The way I understood when I was ready about tin compounds, is that most stannic compounds are readily soluble in a concentrated alkali solution, which in theroy is what we deal with when we introduce tin into nitric acid. This creates a stannic/metastannic acid, then through incineration of the residue then creates stannic oxide, which should be soluble in concentrated sodium hydroxide. I am really trying to make an effort to better understand these chemical compounds/processes, so please correct me if my understanding is wrong.
At this point I am completely stumped, and have run out of ideas, so any thoughts any one else has are more then welcomed???
I had one of the same boards left that the pins came from, so I pulled just over a 1/2lb of them and ran through nitric. I used glondor's SS coffee filter basket technique he described in this thread to recover the foils from the chlorides. It worked perfectly, thanks glondor, I recovered and processed 2.18g from 0.65lbs of pins. I did this just make sure I wasn't going crazy.
I'll stop rambling now, thanks in advance for any input,
Chris
Geo
Well-known member
there is an instance of getting a negative result when gold is present. if you are testing a solution with free oxidizer, it can redissolve the purple test color almost as fast as it appears. Harold pointed this out to me. watch the test carefully and see if it turns purple and instantly clears, like a flash of color. if not, there may not be any gold there.
maynman1751
Well-known member
Without going back through the whole post, have you tried cementing out the values?
Have you tried evaporating the solution down to a syrup and acidifying with strong H2SO4?
Have you tried evaporating the solution down to a syrup and acidifying with strong H2SO4?
Hey Geo, I've had the disappearing stannous stain before, I always try to watch for it when I feel there is an excess of oxidizers.
Palladium, I've read your thread what feels like a hundred times,I tried to follow the procedure you used and I can't see anything you've done that I haven't. I forgot to mention in my previous post that I have tried Hcl/Cl with no positive results.
Maynman, H2so4 is one of the few things I hadn't tried at this point, so I said what the. Heck and added a 100 MLS of H2So4 and a little heat, this is what the solution looks like now,
And this is after diluting and filtering,
The addition of sulfuric also reduced the amount of poewders by about half. I think I mayjust have to donate this one to science, and accept the fact that the gold is gone or just not in the powders anymore. Any experiments you guys have wanted to try let me know I'll give anything a shot at this point?
thanks,
Chris
Palladium, I've read your thread what feels like a hundred times,I tried to follow the procedure you used and I can't see anything you've done that I haven't. I forgot to mention in my previous post that I have tried Hcl/Cl with no positive results.
Maynman, H2so4 is one of the few things I hadn't tried at this point, so I said what the. Heck and added a 100 MLS of H2So4 and a little heat, this is what the solution looks like now,
And this is after diluting and filtering,
The addition of sulfuric also reduced the amount of poewders by about half. I think I mayjust have to donate this one to science, and accept the fact that the gold is gone or just not in the powders anymore. Any experiments you guys have wanted to try let me know I'll give anything a shot at this point?
thanks,
Chris
maynman1751
Well-known member
It definitely looks colloidal.....doesn't it?!!!!!
Ask Butcher. He has some ideas on colloidal gold recovery.
Did you evaporate it down before adding the H2SO4?
Ask Butcher. He has some ideas on colloidal gold recovery.
Did you evaporate it down before adding the H2SO4?
qst42know
Well-known member
There are a couple possibilities in this thread.
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=12496&p=123991&hilit=colloidal#p123991
Was that concentrated sulfuric you added, and did you bring it to a boil?
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=12496&p=123991&hilit=colloidal#p123991
Was that concentrated sulfuric you added, and did you bring it to a boil?
maynman1751 said:
It does look colloidal and that was my first reaction, but here is there thing, I did not add the sulfuric to a solution. I have not been able to keep any gold in a solution, so I added the concentrated sulfuric acid to the solid powders. It instantly turned that purple color and reduced the powders by half as well as changed the powders color from a light tan to an off grey.
qst42know said:
Yes it was concentrated sulfuric and I brought just short of a boil then backed off the heat and let it cool down. I also took a small sample in a test tube and added eight drops of Hcl and one drop of nitric. There was no reaction at first, so I added a little heat and it turned a nice crystal yellow and tested with stannous and got a negative. So I added a little ferrous sulfate to see what would happen, about 8-10 crystals of ferrous and a little dusty brown swirl would form above it and disappear. So I added more ferrous sulfate and it wouldn't produce the same swirl anymore, the solution in the test tube just turned orange. I am NOT all that confident the brown swirl was gold due to a negative stannous test, I know excess oxidizer may have redissolved it. So I added a prill of urea then ferrous and there was still no reaction. So I'm not sure what the reaction was in the test tube was or what the purple sulfuric solution is but I have set the "purple drink" aside for now just in case. And I still have a beaker with unknown powders and chlorides.
This situation is an anomaly wrapped in an enigma rolled in a conundrum, :shock: :shock: :shock:
Chris
maynman1751
Well-known member
WOW! Far out man! I've been there! :mrgreen:
I am a little lost of where your at with this, it does look like gold colloids, and if this was from adding H2SO4 to the white powders, here is my thinking, the solution looks very dilute and to be a large volume, (it also looks like some salts formed of sulfates or chlorides?) with possibly some gold in solution, but gold will not dissolve in H2SO4, and would not form colloids from adding the sulfuric acid to a powder that contained gold.
But if the powders contained chloride salts like NaCl (table salt) and you added H2SO4 you could make HCl gas in solution and if you had tin also in the powders You could have stannous chloride in solution, now if there was some gold in solution you could get the color of purple,
I do not know this is what you have, but it does seem possible,
You may try taking a reasonable size very small sample of this solution, and evaporate it down to a thick syrup, add a little H2SO4, and continue heating (this should drive off any HCl as gas if the solution contains it), it can also help to break the colloids (if this is what the color is from), you may need to repeat the evaporation and sulfuric additions (or you may see black powders form), take care, as the concentrated hot sulfuric is very dangerous (do not boil) do not have heat so high that it boils and splashes hot sulfuric on you and burns you, wear battery gloves and use a face shield, an apron will also be helpful, this is dangerous, so take precautions, once you get the hcl driven off you may see black powders or a black solution in the sulfuric (if gold), let cool and pour the small amount of black solution into a vessel of water to dilute it.
Do not pour water into concentrated sulfuric acid, the water will steam and can splash out acid onto you.
Pour concentrated sulfuric acid into water to dilute it safely.
You may see a black powder of gold form, (if gold was involved), if so decant liquid (if tin was involved it should be soluble as tin sulfate), the black powder (if any) can then be dissolved in HCl with a little bleach (heat to drive off chlorine) and tested with stannous chloride on paper filter or Q-tip or you could use a ferrous sulfate crystal in spot plate to test the solution for gold.
Or the color in the solution in your picture could have come from something else I really do not know.
But if the powders contained chloride salts like NaCl (table salt) and you added H2SO4 you could make HCl gas in solution and if you had tin also in the powders You could have stannous chloride in solution, now if there was some gold in solution you could get the color of purple,
I do not know this is what you have, but it does seem possible,
You may try taking a reasonable size very small sample of this solution, and evaporate it down to a thick syrup, add a little H2SO4, and continue heating (this should drive off any HCl as gas if the solution contains it), it can also help to break the colloids (if this is what the color is from), you may need to repeat the evaporation and sulfuric additions (or you may see black powders form), take care, as the concentrated hot sulfuric is very dangerous (do not boil) do not have heat so high that it boils and splashes hot sulfuric on you and burns you, wear battery gloves and use a face shield, an apron will also be helpful, this is dangerous, so take precautions, once you get the hcl driven off you may see black powders or a black solution in the sulfuric (if gold), let cool and pour the small amount of black solution into a vessel of water to dilute it.
Do not pour water into concentrated sulfuric acid, the water will steam and can splash out acid onto you.
Pour concentrated sulfuric acid into water to dilute it safely.
You may see a black powder of gold form, (if gold was involved), if so decant liquid (if tin was involved it should be soluble as tin sulfate), the black powder (if any) can then be dissolved in HCl with a little bleach (heat to drive off chlorine) and tested with stannous chloride on paper filter or Q-tip or you could use a ferrous sulfate crystal in spot plate to test the solution for gold.
Or the color in the solution in your picture could have come from something else I really do not know.
beav3r316
Active member
I know this is incredibly old, but, I have to know...
Did you ever recover the gold?
And, if so, was it colloidal?
I did have a question too. You said the HCL mix was orange. Iron? Did you check the crushed incinerates with a magnet? (I may have missed that, if so. It's 4 am...but I HAVE to read before bed...)
Again, sorry to bump, but, I found this thread full of good things, had I saw it 5 months ago, it would have saved me some heartache.
Did you ever recover the gold?
And, if so, was it colloidal?
I did have a question too. You said the HCL mix was orange. Iron? Did you check the crushed incinerates with a magnet? (I may have missed that, if so. It's 4 am...but I HAVE to read before bed...)
Again, sorry to bump, but, I found this thread full of good things, had I saw it 5 months ago, it would have saved me some heartache.
beav3r316 said:
The test was left inconclusive and the powders were added to my flux refining drum for pyrorefining in the future. Sorry I couldn't have been of more help. The test was four years ago so my memory is bit fuzzy on it!
cnbarr said:
Knowing you I bet you were hoping to forget this, we have all been there at some point but the thing to remember is that if it isn't a customers material it isn't that much of a worry, you will get that missing gold at some point and look what's happened to its price over time 8)
beav3r316
Active member
cnbarr said:
No worries!
I just saw this thread and was reading through it (as i am trying to do with EVERY thread on grf) and it had some relevant information pertaining to the first batch of pins i tried to do (and failed, as my school of youtube was far from the correct way of doing things).
Great stuff in this thread though, a true wealth of information.
Hope you got the majority of the gold in the end, your persistence is admirable.
Thanks again for sharing
